US20020004023A1 - Chloride assisted hydrometallurgical extraction of metal - Google Patents
Chloride assisted hydrometallurgical extraction of metal Download PDFInfo
- Publication number
- US20020004023A1 US20020004023A1 US09/866,027 US86602701A US2002004023A1 US 20020004023 A1 US20020004023 A1 US 20020004023A1 US 86602701 A US86602701 A US 86602701A US 2002004023 A1 US2002004023 A1 US 2002004023A1
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- Prior art keywords
- pressure oxidation
- copper
- process according
- raffinate
- sulphate
- Prior art date
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- Granted
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 title abstract description 13
- 239000002184 metal Substances 0.000 title abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title description 27
- 230000003647 oxidation Effects 0.000 claims abstract description 42
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 42
- 239000007787 solid Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000010949 copper Substances 0.000 claims abstract description 24
- 229910052802 copper Inorganic materials 0.000 claims abstract description 23
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 21
- 230000008020 evaporation Effects 0.000 claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 20
- 239000012141 concentrate Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000002386 leaching Methods 0.000 claims abstract description 13
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000000638 solvent extraction Methods 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 9
- -1 sulphate ions Chemical class 0.000 claims abstract description 9
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 229910021653 sulphate ion Inorganic materials 0.000 claims abstract description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000003929 acidic solution Substances 0.000 claims abstract description 4
- 230000002378 acidificating effect Effects 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 150000004820 halides Chemical class 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000004064 recycling Methods 0.000 claims description 8
- 239000000446 fuel Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- 150000001879 copper Chemical class 0.000 claims description 3
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims 1
- 150000001805 chlorine compounds Chemical group 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 229910052728 basic metal Inorganic materials 0.000 abstract 3
- 239000002253 acid Substances 0.000 description 15
- 238000001914 filtration Methods 0.000 description 8
- 239000002562 thickening agent Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910052602 gypsum Inorganic materials 0.000 description 3
- 239000010440 gypsum Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2s)-2-aminopentanedioic acid;hydrochloride Chemical class Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 229910001779 copper mineral Inorganic materials 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/043—Sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0423—Halogenated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0476—Separation of nickel from cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- This invention relates to the hydrometallurgical treatment of metal ores or concentrates.
- it relates to the extraction of copper from sulphide ores or other concentrates in the presence of halogen ions, such as chloride ions.
- the purpose of the present invention is to provide an improved process for the extraction of metals from sulphide ores.
- a process for the extraction of copper from a sulphide copper ore or concentrate comprising the steps of subjecting the ore or concentrate to pressure oxidation in the presence of oxygen and an acidic solution containing halide and sulphate ions to obtain a resulting pressure oxidation slurry, subjecting the slurry to a liquid/solid separation step to obtain a resulting pressure oxidation filtrate and a solid residue containing an insoluble basic copper sulphate salt; leaching the basic copper sulphate salt produced by the pressure oxidation with an acidic sulphate solution in a second leaching to dissolve the basic copper salt to produce a leach liquor containing copper sulphate in solution and a resulting solid residue; separating the leach liquor from the solid residue; subjecting the leach liquor to a solvent extraction process to produce copper concentrate solution and a copper depleted raffinate; recycling at least a portion of the raffinate to the pressure oxidation; and wherein the
- concentrate in this specification refers to any material in which the metal value content has been increased to a higher percentage by weight as compared with the naturally occurring ore and includes man made artificial sulphide ore, such as matte, and metal values precipitated as solids such as hydroxides and sulphides.
- FIG. 1 is a flow diagram of a hydrometallurgical metal extraction process according to one embodiment of the invention.
- FIG. 2 is a flow diagram of a hydrometallurgical metal extraction process according to another embodiment of the invention.
- the feed ore or concentrate to the process may contain one or more sulphide minerals of the base metals Cu, Ni, Co and Zn, frequently combined with Fe and sometimes with other elements, such as As, Sb, and Ag.
- reference numeral 10 generally indicates a hydrometallurgical process according to one embodiment of the invention.
- the process 10 comprises a pressure oxidation stage 12 , an atmospheric leach 14 , a liquid/solid separation 24 , a solvent extraction 16 , an evaporation stage 20 and a neutralization 22 .
- the copper concentrate Prior to the pressure oxidation stage 12 , the copper concentrate is first subjected to a regrind to reduce the particle size to about 2 %+325 mesh.
- the concentrate is subjected to the pressure oxidation 12 in an autoclave in the presence of an acidic solution containing sulphate, chloride and preferably copper ions.
- the amount of acid introduced into the pressure oxidation 12 is sufficient to maintain the discharge solution from the autoclave, when operated in a continuous mode, at a pH of above 2.0, typically pH 2.3-3.8.
- the chloride ion concentration in the solution in the autoclave is maintained at about 8-20 g/L, preferably about 12 g/L.
- the pressure oxidation 12 is carried out at a temperature of from about 115° C. to about 175° C., preferably about 130° C. to about 155° C., under a pressure of about 100-300 psig. This is total pressure comprising oxygen pressure plus steam pressure.
- the retention time is about 0.5-2.5 hours and the process is normally carried out in a continuous fashion in the autoclave. However, the process can also be carried out in a batch-wise fashion, if desired.
- the solids content in the autoclave is maintained at about 12-25%, i.e. 150-300 g/L solids as determined by the heat balance and viscosity limitations.
- the slurry produced in the autoclave is discharged through a series of one or more flash tanks (not shown) to reduce the pressure to atmospheric pressure and the temperature to about 90-100° C.
- the liquid part of the slurry is referred to as the product solution from the pressure oxidation stage 12 and is indicated by reference numeral 21 .
- the solids from the pressure oxidation stage 12 after the filtration 24 are treated in the atmospheric leaching stage 14 at about pH 1.2 to pH 2.2 using raffinate from the solvent extraction 16 , which is acidic, to dissolve the basic copper sulphate.
- the leaching 14 takes place at a temperature of about 40° C. for a retention time of about 15-60 minutes.
- the percentage solids in the feed to the leach 14 is typically about 3-15% or about 30-170 g/L, although it is possible to operate the process outside this range.
- the percentage solids drops substantially during the leach 14 as the basic copper sulphate dissolves.
- the product g/L solids may be as little as one half of the feed g/L solids.
- the basic copper salts dissolve almost completely with very little of the iron present in the concentrate going into solution, provided care is taken to maintain the pH in the range 1.2 to 2.2, preferably pH 1.5 to 2.0.
- the slurry 31 from the atmospheric leaching stage 14 is sometimes difficult if not impossible to filter, but settles well.
- the slurry 31 is pumped to a counter current decantation (CCD) wash circuit 34 .
- CCD counter current decantation
- the solids are fed through a series of thickeners with wash water added in the opposite direction.
- wash water added in the opposite direction.
- the solids are washed and entrained solution removed, together with the soluble metals dissolved therein.
- About 3 to 7 thickeners are required with a wash ratio (water to solids) of about 2 to 5 to reduce entrained liquor down to less than 100 ppm dissolved Cu in the final residue.
- the thickener underflow from the last thickener is the final residue stream 35 at about 50% solids. This can be treated for the recovery of precious metals, such as gold and silver, or sent to tailings.
- the main constituents of the stream 35 are hematite and elemental sulphur, which may also be recovered by a combination of other processes, such as flotation and leaching into a specific solvent for sulphur, e.g. perchloroethylene, if market conditions warrant.
- the thickener overflow from the first thickener is the product solution 33 which is fed to the solvent extraction stage 16 , as shown.
- Copper is extracted from the product solution 33 from the CCD circuit 34 in two stages of extraction in the solvent extraction stage 16 to produce a raffinate 37 .
- the raffinate 37 is split, as indicated at 38 , into three streams 40 , 41 and 42 .
- the stream 40 which comprises about 2 ⁇ 3 of the raffinate 37 is recycled to effect the atmospheric leach 14 , as indicated above.
- the actual volume of 40 is determined by the acid needs of the leach 14 , to dissolve the basic copper sulphate as described, and maintain a slight excess of acid, i.e. pH 1.5-2.0 which corresponds to about 1-5 g/L H 2 SO 4 .
- the acid requirements for stream 40 are less than the total acid contained in 37 , and part of the remainder is used in the pressure oxidation 12 as an acid source for the reactions therein. This is supplied by stream 42 .
- streams 41 and 42 are each about 1 ⁇ 6 of 37 .
- the stream 41 which comprises about 1 ⁇ 6 of the raffinate 37 is subjected to the neutralization 22 with lime rock and after liquid/solid separation 43 results in gypsum, which can be discarded, and wash water which is recycled as wash water to the CCD wash circuit 34 .
- the amount of water to be evaporated must be minimized.
- the copper concentration in the stream 31 is maintained at a more concentrated level, i.e. at about 35 g/L, compared with a value of 12 g/L in the absence of evaporation. This in turn generates a more concentrated acid stream 42 containing about 48 g/L H 2 SO 4 instead of only 18 g/L H 2 SO 4 .
- Direct fired evaporators do not have the advantage of multiple effect of the steam generated which can generally reduce fuel costs in indirect evaporators, and thus justify evaporating large volume of water.
- the process 100 also comprises a pressure oxidation stage 12 , filtration 24 , atmospheric leach 14 , CCD wash circuit 34 , solvent extraction 16 , evaporation 20 and neutralization 22 .
- the liquid 21 from the filtration 24 is subjected to a copper solvent extraction 50 in order to recover copper values therefrom.
- the filtration 24 is the separation point between the high chloride liquid used in the pressure oxidation 12 , which liquid is recycled as indicated, and a low chloride or chloride free liquid going to the atmospheric leach 14 .
- the filtration 24 is always accompanied by a wash with water or recycled low chloride water or a concentration of both to remove as much chloride from the solids (filter cake) as possible.
- the objective is to minimize transfer of chloride from the high chloride circuit to the low chloride circuit, to counteract chloride build up in the latter circuit.
- the stream 42 is subjected to the evaporation 20 , as described with reference to FIG. 1, prior to recycle to the pressure oxidation 12 .
- there is no need to recycle acid from the low chloride circuit because enough acid is generated by the copper solvent extraction 50 in the form of raffinate 63 .
- the neutralization product is subject to a liquid/solid separation step to produce solid gypsum which can be discarded and a liquid 66 which is subjected to the evaporation 20 before recycle.
- the raffinate 37 from the solvent extraction 16 is split into only two streams, i.e. 2 ⁇ 3 into stream 40 which is used in the atmospheric leach 14 , and 1 ⁇ 3 into stream 41 which is subjected to the neutralization 22 and liquid/solid separation 43 to produce solid gypsum which can be discarded and a stream 45 which is split, as indicated at 46 into a stream which is recycled as wash water to the CCD circuit 34 and stream 42 which goes to the evaporation 20 for recycle to the pressure oxidation 12 .
- This serves to recycle chloride from the low chloride circuit back to the high chloride circuit.
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Abstract
A process for the extraction of copper from a sulphide ore or concentrate comprises the steps of subjecting the ore or concentrate to pressure oxidation in the presence of oxygen and an acidic solution containing halide and sulphate ions to obtain a resulting pressure oxidation slurry. The slurry is subjected to a liquid/solid separation step to obtain a resulting pressure oxidation filtrate and a solid residue containing an insoluble basic metal sulphate salt. The basic metal sulphate salt is leached in a second leaching with an acidic sulphate solution to dissolve the basic metal salt to produce a leach liquor containing a metal sulphate, e.g. copper sulphate, in solution and a resulting solid residue. The leach liquor is separated from the solid residue and subjected to a solvent extraction process to produce metal concentrate solution and a metal depleted raffinate. At least a portion of the raffinate is recycled to the pressure oxidation after being subjected to evaporation.
Description
- This application is a division of U.S. patent application Ser. No. 09/452,431 filed Dec. 1, 1999 which in turn is a division of U.S. patent application Ser. No. 08/911,797 filed Aug. 15, 1997. The contents of the foregoing applications are incorporated herein by reference.
- This invention relates to the hydrometallurgical treatment of metal ores or concentrates. In particular, it relates to the extraction of copper from sulphide ores or other concentrates in the presence of halogen ions, such as chloride ions.
- The hydrometallurgical treatment of sulphide concentrates whereby the concentrate is subjected to pressure oxidation in the presence of chloride ions is known. See for example U.S. Pat. Nos. 4,039,406; 5,645,708; and 5,650,057.
- The purpose of the present invention is to provide an improved process for the extraction of metals from sulphide ores.
- According to the invention there is provided a process for the extraction of copper from a sulphide copper ore or concentrate, comprising the steps of subjecting the ore or concentrate to pressure oxidation in the presence of oxygen and an acidic solution containing halide and sulphate ions to obtain a resulting pressure oxidation slurry, subjecting the slurry to a liquid/solid separation step to obtain a resulting pressure oxidation filtrate and a solid residue containing an insoluble basic copper sulphate salt; leaching the basic copper sulphate salt produced by the pressure oxidation with an acidic sulphate solution in a second leaching to dissolve the basic copper salt to produce a leach liquor containing copper sulphate in solution and a resulting solid residue; separating the leach liquor from the solid residue; subjecting the leach liquor to a solvent extraction process to produce copper concentrate solution and a copper depleted raffinate; recycling at least a portion of the raffinate to the pressure oxidation; and wherein the raffinate is subjected to evaporation to remove water therefrom prior to the recycle thereof; and wherein the evaporation is effected by means of a direct-fired evaporation process comprising the submerged combustion of a fuel in the raffinate being recycled.
- The term “concentrate” in this specification refers to any material in which the metal value content has been increased to a higher percentage by weight as compared with the naturally occurring ore and includes man made artificial sulphide ore, such as matte, and metal values precipitated as solids such as hydroxides and sulphides.
- Further objects and advantages of the invention will become apparent from the description of preferred embodiments of the invention below.
- FIG. 1 is a flow diagram of a hydrometallurgical metal extraction process according to one embodiment of the invention.
- FIG. 2 is a flow diagram of a hydrometallurgical metal extraction process according to another embodiment of the invention.
- The feed ore or concentrate to the process may contain one or more sulphide minerals of the base metals Cu, Ni, Co and Zn, frequently combined with Fe and sometimes with other elements, such as As, Sb, and Ag.
- In FIG. 1,
reference numeral 10 generally indicates a hydrometallurgical process according to one embodiment of the invention. Theprocess 10 comprises apressure oxidation stage 12, anatmospheric leach 14, a liquid/solid separation 24, asolvent extraction 16, anevaporation stage 20 and aneutralization 22. - Prior to the
pressure oxidation stage 12, the copper concentrate is first subjected to a regrind to reduce the particle size to about 2 %+325 mesh. - The concentrate is subjected to the
pressure oxidation 12 in an autoclave in the presence of an acidic solution containing sulphate, chloride and preferably copper ions. - The amount of acid introduced into the pressure oxidation12 (by way of recycle after the initial startup, as will be described below) is sufficient to maintain the discharge solution from the autoclave, when operated in a continuous mode, at a pH of above 2.0, typically pH 2.3-3.8.
- The chloride ion concentration in the solution in the autoclave is maintained at about 8-20 g/L, preferably about 12 g/L.
- The
pressure oxidation 12 is carried out at a temperature of from about 115° C. to about 175° C., preferably about 130° C. to about 155° C., under a pressure of about 100-300 psig. This is total pressure comprising oxygen pressure plus steam pressure. - The retention time is about 0.5-2.5 hours and the process is normally carried out in a continuous fashion in the autoclave. However, the process can also be carried out in a batch-wise fashion, if desired.
- In the
pressure oxidation stage 12, all copper minerals are converted to basic copper sulphate CuSO4·2Cu(OH)2, i.e. all the copper being recovered reports to the solid phase in thepressure oxidation 12. - The solids content in the autoclave is maintained at about 12-25%, i.e. 150-300 g/L solids as determined by the heat balance and viscosity limitations.
- The slurry produced in the autoclave is discharged through a series of one or more flash tanks (not shown) to reduce the pressure to atmospheric pressure and the temperature to about 90-100° C. The liquid part of the slurry is referred to as the product solution from the
pressure oxidation stage 12 and is indicated byreference numeral 21. - The slurry from the flash tank(s)22 is filtered, as shown at 24, and the resultant filter cake is washed thoroughly to remove entrained liquor as much as possible.
- The solids from the
pressure oxidation stage 12 after thefiltration 24, are treated in theatmospheric leaching stage 14 at about pH 1.2 to pH 2.2 using raffinate from thesolvent extraction 16, which is acidic, to dissolve the basic copper sulphate. Theleaching 14 takes place at a temperature of about 40° C. for a retention time of about 15-60 minutes. The percentage solids in the feed to theleach 14 is typically about 3-15% or about 30-170 g/L, although it is possible to operate the process outside this range. The percentage solids drops substantially during theleach 14 as the basic copper sulphate dissolves. Thus, the product g/L solids may be as little as one half of the feed g/L solids. - During the
atmospheric leaching stage 14, the basic copper salts dissolve almost completely with very little of the iron present in the concentrate going into solution, provided care is taken to maintain the pH in the range 1.2 to 2.2, preferably pH 1.5 to 2.0. - The
slurry 31 from theatmospheric leaching stage 14 is sometimes difficult if not impossible to filter, but settles well. In view of the need to wash the leach solids very thoroughly, theslurry 31 is pumped to a counter current decantation (CCD)wash circuit 34. In theCCD circuit 34, the solids are fed through a series of thickeners with wash water added in the opposite direction. By this method, the solids are washed and entrained solution removed, together with the soluble metals dissolved therein. About 3 to 7 thickeners (not shown) are required with a wash ratio (water to solids) of about 2 to 5 to reduce entrained liquor down to less than 100 ppm dissolved Cu in the final residue. - The thickener underflow from the last thickener is the
final residue stream 35 at about 50% solids. This can be treated for the recovery of precious metals, such as gold and silver, or sent to tailings. - The main constituents of the
stream 35 are hematite and elemental sulphur, which may also be recovered by a combination of other processes, such as flotation and leaching into a specific solvent for sulphur, e.g. perchloroethylene, if market conditions warrant. - The thickener overflow from the first thickener is the
product solution 33 which is fed to thesolvent extraction stage 16, as shown. - Copper is extracted from the
product solution 33 from theCCD circuit 34 in two stages of extraction in thesolvent extraction stage 16 to produce a raffinate 37. - The raffinate37 is split, as indicated at 38, into three
streams stream 40 which comprises about ⅔ of the raffinate 37 is recycled to effect theatmospheric leach 14, as indicated above. The actual volume of 40 is determined by the acid needs of theleach 14, to dissolve the basic copper sulphate as described, and maintain a slight excess of acid, i.e. pH 1.5-2.0 which corresponds to about 1-5 g/L H2SO4. The acid requirements forstream 40 are less than the total acid contained in 37, and part of the remainder is used in thepressure oxidation 12 as an acid source for the reactions therein. This is supplied bystream 42. Any acid still left over from 37, not used by 40 or 42, is considered excess, and is neutralized. This isstream 41. Typicallystreams stream 41 which comprises about ⅙ of the raffinate 37 is subjected to theneutralization 22 with lime rock and after liquid/solid separation 43 results in gypsum, which can be discarded, and wash water which is recycled as wash water to theCCD wash circuit 34. - The
liquid 21 from thefiltration 24, along with thestream 42, is subjected to theevaporation 20 to remove water and produce a more concentrated acid andchloride solution 44 which is recycled to thepressure oxidation 12. - The evaporation of the solution prior to recycling is problematical due to the very corrosive nature thereof, i.e. high acidity (50 g/L free acid), high chloride content (12 g/L) and high temperature in evaporation. This precludes the use of most if not all commercially available evaporators, which are normally based on indirect heat transfer through thin metal surfaces, such as shell and tube evaporators made typically of stainless steel. Titanium would be suitable but is too expensive if used in the large quantities which would be required for this type of application.
- However, the problem has been solved by direct-fired evaporation using submerged combustion of a fuel in the
solution 44 and using titanium material. - In order to keep the size of the evaporator down, and minimize operating and capital costs, the amount of water to be evaporated must be minimized. In order to achieve this, the copper concentration in the
stream 31 is maintained at a more concentrated level, i.e. at about 35 g/L, compared with a value of 12 g/L in the absence of evaporation. This in turn generates a moreconcentrated acid stream 42 containing about 48 g/L H2SO4 instead of only 18 g/L H2SO4. This effectively reduces the volume of the water to be evaporated by putting the same mass of acid in a smaller volume of water, thus reducing the size of the evaporator, hence justifying the use of titanium, and the fuel costs necessary to operate a direct fired evaporator. Direct fired evaporators do not have the advantage of multiple effect of the steam generated which can generally reduce fuel costs in indirect evaporators, and thus justify evaporating large volume of water. - With reference to FIG. 2, a
process 100 according to another embodiment of the invention is shown. - The
process 100 also comprises apressure oxidation stage 12,filtration 24,atmospheric leach 14,CCD wash circuit 34,solvent extraction 16,evaporation 20 andneutralization 22. - In the
process 100 some of the metal values being recovered also report to thepressure oxidation liquid 21 in addition to the solid, which solid is subjected to theatmospheric leach 14 as described with reference to FIG. 1. - The liquid21 from the
filtration 24 is subjected to acopper solvent extraction 50 in order to recover copper values therefrom. - It should be noted that although the
step 24 is referred to as a filtration, any suitable liquid/solid separation method can be employed. - The
filtration 24 is the separation point between the high chloride liquid used in thepressure oxidation 12, which liquid is recycled as indicated, and a low chloride or chloride free liquid going to theatmospheric leach 14. Thefiltration 24 is always accompanied by a wash with water or recycled low chloride water or a concentration of both to remove as much chloride from the solids (filter cake) as possible. The objective is to minimize transfer of chloride from the high chloride circuit to the low chloride circuit, to counteract chloride build up in the latter circuit. - However, despite the washing of the solid residue produced by the
filtration 24, the chloride concentration is prone to increase in the low chloride circuit, because it is essentially a dead ended circuit with minimum bleed. - This problem has been overcome by recycling a stream from the low chloride circuit to the high chloride circuit. This stream is indicated by
reference numeral 42 in FIG. 2 to correspond with thestream 42 in FIG. 1 which also comprises a recycle from the low chloride circuit to the high chloride circuit. - Again the
stream 42 is subjected to theevaporation 20, as described with reference to FIG. 1, prior to recycle to thepressure oxidation 12. However, in this case, there is no need to recycle acid from the low chloride circuit because enough acid is generated by thecopper solvent extraction 50 in the form of raffinate 63. In fact, it is usually necessary to neutralize some of the acid in the raffinate 63, as indicated at 64 prior to recycling the raffinate 63. As indicated at 65, the neutralization product is subject to a liquid/solid separation step to produce solid gypsum which can be discarded and a liquid 66 which is subjected to theevaporation 20 before recycle. - Since there is no need to recycle acid from the low chloride circuit, the
raffinate 37 from thesolvent extraction 16 is split into only two streams, i.e. ⅔ intostream 40 which is used in theatmospheric leach 14, and ⅓ intostream 41 which is subjected to theneutralization 22 and liquid/solid separation 43 to produce solid gypsum which can be discarded and a stream 45 which is split, as indicated at 46 into a stream which is recycled as wash water to theCCD circuit 34 andstream 42 which goes to theevaporation 20 for recycle to thepressure oxidation 12. This serves to recycle chloride from the low chloride circuit back to the high chloride circuit. - While only preferred embodiments of the invention have been described herein in detail, the invention is not limited thereby and modifications can be made within the scope of the attached claims.
Claims (14)
1. A process for the extraction of copper from a sulphide copper ore or concentrate, comprising the steps of:
subjecting the ore or concentrate to pressure oxidation in the presence of oxygen and an acidic solution containing halide and sulphate ions to obtain a resulting pressure oxidation slurry, subjecting the slurry to a liquid/solid separation step to obtain a resulting pressure oxidation filtrate and a solid residue containing an insoluble basic copper sulphate salt;
leaching the basic copper sulphate salt produced by the pressure oxidation with an acidic sulphate solution in a second leaching to dissolve the basic copper salt to produce a leach liquor containing copper sulphate in solution and a resulting solid residue;
separating the leach liquor from the solid residue;
subjecting the leach liquor to a solvent extraction process to produce copper concentrate solution and a copper depleted raffinate;
recycling at least a portion of the raffinate to the pressure oxidation; and wherein
the raffinate is subjected to evaporation to remove water therefrom prior to the recycle thereof; and wherein
the evaporation is effected by means of a direct-fired evaporation process comprising the submerged combustion of a fuel in the raffinate being recycled.
2. The process according to claim 1 , further comprising the steps of splitting the raffinate in at least two portions, wherein the one portion is recycled to the pressure oxidation and the other portion is recycled to the second leaching.
3. The process according to claim 1 , further comprising the step of recycling the pressure oxidation filtrate to the pressure oxidation.
4. The process according to claim 3 , further comprising the step of subjecting the pressure oxidation filtrate to evaporation to remove water therefrom prior to the recycle thereof to the pressure oxidation.
5. The process according to claim 4 , wherein the evaporation is effected by means of a direct-fired evaporation process comprising the submerged combustion of a fuel in the filtrate being recycled.
6. A process according to claim 3 , further comprising the steps of subjecting the pressure oxidation filtrate to a solvent extraction process, prior to the recycling of the filtrate, to produce a further copper concentrate solution and a further copper depleted raffinate which further copper depleted raffinate is recycled to the pressure oxidation.
7. The process according to claim 6 , further comprising the step of subjecting the further copper depleted raffinate to neutralization prior to the recycling thereof to the pressure oxidation.
8. The process according to claim 1 , wherein the pressure oxidation is carried out at a pH value of above about 2.
9. The process according to claim 8 , wherein the pH in the pressure oxidation is from about 2.3 to about 3.8.
10. The process according to claim 1 , wherein the second leaching is effected at a pH in the range of about 1.2 to about 2.2.
11. The process according to claim 10 , wherein the pH in the second leaching is from about 1.5 to about 2.0.
12. The process according to claim 1 , wherein the pressure oxidation slurry is flashed to atmospheric pressure at a temperature below the melting point of elemental sulphur.
13. The process according to claim 1 , wherein the halide is selected from chloride and bromide.
14. The process according to claim 1 , wherein the copper concentration in the leach liquor is maintained at a value of about 35 g/L.
Priority Applications (1)
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US09/866,027 US6455019B2 (en) | 1997-08-15 | 2001-05-25 | Process for the extraction of copper from a sulphide copper ore or concentrate |
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US45243199A | 1999-12-01 | 1999-12-01 | |
US09/866,027 US6455019B2 (en) | 1997-08-15 | 2001-05-25 | Process for the extraction of copper from a sulphide copper ore or concentrate |
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US09/866,027 Expired - Lifetime US6455019B2 (en) | 1997-08-15 | 2001-05-25 | Process for the extraction of copper from a sulphide copper ore or concentrate |
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US20160331380A1 (en) * | 2014-01-10 | 2016-11-17 | Nanyang Technological University | Embolic device, an apparatus for embolizing a target vascular site and a method thereof |
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